EP2773706B1 - Dispositif hydrophile de transport de fluide - Google Patents

Dispositif hydrophile de transport de fluide Download PDF

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Publication number
EP2773706B1
EP2773706B1 EP12783802.7A EP12783802A EP2773706B1 EP 2773706 B1 EP2773706 B1 EP 2773706B1 EP 12783802 A EP12783802 A EP 12783802A EP 2773706 B1 EP2773706 B1 EP 2773706B1
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Prior art keywords
hydrophilic
layer
nanoparticles
fluid
article
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German (de)
English (en)
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EP2773706A1 (fr
Inventor
Raymond J. Kenney
Theresa J. GERTEN
Daniel P. DECABOOTER
Naiyong Jing
Garry W. LACHMANSINGH
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3M Innovative Properties Co
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3M Innovative Properties Co
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/056—Forming hydrophilic coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B01L2300/0627—Sensor or part of a sensor is integrated
    • B01L2300/0645—Electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0809—Geometry, shape and general structure rectangular shaped
    • B01L2300/0816—Cards, e.g. flat sample carriers usually with flow in two horizontal directions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/0864—Configuration of multiple channels and/or chambers in a single devices comprising only one inlet and multiple receiving wells, e.g. for separation, splitting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/16—Surface properties and coatings
    • B01L2300/161—Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0406—Moving fluids with specific forces or mechanical means specific forces capillary forces
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems

Definitions

  • the present disclosure relates to hydrophilic articles, including those capable of providing fluid transport. Articles incorporating hydrophilic layers including sintered, acidified nanoparticles are described. The present disclosure also relates to methods of making and using hydrophilic fluid transport articles.
  • WO 2011/124906 A1 relates to a sampling plate for measuring certain selected properties of a liquid sample.
  • the sample plate has a sample zone for receiving a liquid sample which is surrounded by an air porous body.
  • the air porous body acts to receive air from the sample zone as it is displaced by an incoming liquid sample, thereby allowing efficient spreading of the liquid sample.
  • US 2011/0033694 A1 relates to a coated article having a substrate coated with a layer of silica nanoparticles. The coating is substantially uniform in thickness, durably adheres to the substrate, and provides antireflection and/or hydrophilic surface properties to the substrate.
  • the present disclosure provides a hydrophilic article comprising a substrate, a first surface of a hydrophilic layer comprising sintered, acidified silica nanoparticles attached to the substrate, and a spacer layer attached to a first portion of a second surface of the hydrophilic layer opposite the first surface.
  • the spacer layer defines at least one fluid transport channel bounded on one side by a second portion of the hydrophilic layer.
  • the hydrophilic article further comprises a cover layer attached to the spacer layer and covering at least a portion of the fluid transport channel.
  • the fluid transport channel comprises a landing zone comprising an exposed portion of the hydrophilic layer.
  • the fluid transport channel comprises a detection zone.
  • the hydrophilic article comprises a cover layer in contact with at least a portion of a surface of the spacer layer opposite the hydrophilic layer, e.g., a cover layer comprising a second hydrophilic layer comprising sintered, acidified silica nanoparticles attached to a second substrate.
  • the nanoparticles comprise elongated silica nanoparticles having an average length to diameter ratio of at least 2, e.g., 3 to 15. In some embodiments, the nanoparticles comprise substantially spherical silica nanoparticles having a ratio of maximum diameter to minimum diameter of less than 2, e.g., less than 1.2. In some embodiments, the nanoparticles comprise 50 to 95 weight percent substantially spherical silica nanoparticles having a ratio of maximum diameter to minimum diameter of less than 2, and 5 to 50 parts by weight elongated silica nanoparticles having an average length to diameter ratio of at least 2, based on the total weight of the nanoparticles.
  • the hydrophilic layer comprises at least 95 weight percent of the nanoparticles. In some embodiments, the hydrophilic layer comprises no greater than 5 weight percent resin. In some embodiments, the hydrophilic layer consists essentially of the nanoparticles.
  • the present disclosure provides a method of transporting a fluid with a hydrophilic article of the present disclosure.
  • Such methods comprise applying the fluid to a first region of the second portion of the second surface of the hydrophilic layer and wicking the fluid within the fluid transport channel from the first region to a second region of the second portion of the second surface of the hydrophilic layer.
  • the fluid is a biological fluid.
  • fluidic diagnostic test devices conduct fluid from a first position to a second position, e.g. from a source to a detection region of the device.
  • fluidic diagnostic test devices include a substrate made from one or more materials selected to provide certain desirable qualities to the device.
  • substrates often include polymeric films, which provide desired mechanical properties.
  • polymeric films are hydrophobic and do not promote transport of fluids, particularly aqueous solutions such as bodily fluids, to an extent sufficient to provide the device with a desired level of performance. Therefore, most polymeric films require some form of surface treatment or coating to render them sufficiently hydrophilic to provide fluid transport.
  • Products suitable for fluid transport applications can be produced using surfactant-containing systems.
  • a surfactant coating on at least a portion of the substrate can provide physical or chemical properties that promote fluid transport and, therefore, improve performance of the device.
  • the use of surfactants can result in undesirable attributes.
  • some surfactant chemistries impart haze, which can be undesirable, particularly in applications designed for diagnostic devices that rely on optical interrogation methods.
  • surfactants tend to be fugitive and the hydrophilicity they impart can diminish with time; thus, limiting the product's shelf life.
  • the fugitive nature of the surfactants can also lead to contamination of fluids contacting them during use and interfere with subsequent analyses of such fluids.
  • surfactant contamination can interfere with the chemical or electrochemical assay detection in devices using hydrophilic films as capillary flow devices, e.g., diabetes glucose monitors and their associated test strips.
  • adhesives including pressure sensitive adhesives, to many surfactant-containing coatings.
  • a hydrophilic layer can be prepared from sintered, acidified silica nanoparticles.
  • the hydrophilic layer is substantially surfactant-free.
  • a surfactant is an amphiphilic organic compound.
  • a surfactant-free material would not contain any amphiphilic organic compounds. However, as a practical matter this may be difficult or impossible to achieve. For example, trace amounts of such materials may be present in purchased or manufactured raw materials, or may arise as contaminants in a particular manufacturing process.
  • a material is "substantially surfactant-free” if it contains less than 0.002 wt.% amphiphilic organic compounds based on the total weight of the material. In some embodiments, substantially surfactant-free materials contain no greater than 0.001 wt.% or even no greater than 0.0005 wt.% amphiphilic organic compounds based on the total weight of the material
  • Hydrophilic article 100 comprises substrate 110, hydrophilic layer 120, and spacer layer 130. Generally, hydrophilic layer 120 is located between substrate 110 and spacer layer 130.
  • hydrophilic layer 120 is directly attached to first surface 112 of substrate 110. In some embodiments, hydrophilic layer 120 may be indirectly attached to substrate 110, i.e., one or more additional layers, e.g., adhesive layers or primer layers, may be located between the hydrophilic layer and the substrate.
  • additional layers e.g., adhesive layers or primer layers
  • hydrophilic layer 120 may be directly attached to first surface 132 of spacer layer 130.
  • hydrophilic layer 120 may be indirectly attached to spacer layer 130, i.e., one or more additional layers, e.g., adhesive layers or primer layers, may be located between the hydrophilic layer and the spacer layer.
  • spacer layer 130 only covers a portion of the hydrophilic layer.
  • the gaps in coverage create fluid transport channel 140.
  • Fluid transport channel 140 is bounded on one side by the surface of hydrophilic layer 120 left exposed by the gaps in coverage by the spacer layer.
  • the exposed edges of spacer layer 130 create the walls 135 defining the boundaries of fluid transport channel 140.
  • walls 135 constrain fluid with the fluid transport channel.
  • hydrophilic layer 120 facilitates the transport along the channel between walls 135, and substantially prevents the flow of fluid under spacer layer 130.
  • the fluid transport channel can have any dimensions and may take on any configuration suitable for the intended application.
  • FIGS. 2 and 3 illustrate one exemplary fluid transport channel containing certain generic features that may be beneficial in certain applications. Particular features illustrated in FIGS. 2 and 3 may be used alone or in combination with other features, including unillustrated features.
  • fluid transport channel 140 includes landing zone 150.
  • landing zone means a location allowing fluid to be introduced into the fluid transport channel.
  • the landing zone may be located at an edge of the hydrophilic article.
  • landing zone 150 is proximate edge 105 of hydrophilic article 100.
  • fluid can be introduced into fluid transport channel 140 by simply contacting the fluid with landing zone 150, e.g., by contacting edge 105 with the fluid.
  • the open area in spacer layer 130 at edge 105 permits fluid to contact landing zone 150 and enter fluid transport channel 140.
  • the landing zone is located at a position away from the edge of the article. Regardless of its location, in some embodiments, the landing zone may be covered or otherwise protected from fluid contact until use. In such embodiments, it may be necessary to breach such a cover, e.g., by piercing or removing at least a portion of the cover to expose the landing zone to fluid.
  • fluid transport channel 140 defines a path for fluid to travel by capillary action along hydrophilic layer 120 from a landing zone to another desired location, e.g., detection zones 170 and 175.
  • detection zone refers to a location in the fluid path where one or more properties of the fluid can be detected.
  • a detection zone may be a location where the fluid can be optically interrogated.
  • light UV, IR, visible, and the like
  • the fluids interaction with the light e.g., absorption, scatter, reflection, and the like
  • an electrochemical sensor may be used for detection.
  • An electrochemical sensor is a device configured to detect the presence of, and/or measure the concentration of, an analyte by way of electrochemical oxidation and reduction reactions within the sensor.
  • the hydrophilic article includes an electrode system comprising a set of measuring electrodes, e.g., at least a working electrode and a counter electrode, within the detection zone.
  • the detection zone may be configured such that sample fluid entering the chamber is placed in electrolytic contact with both the working electrode and the counter electrode. This allows electrical current to flow between the measuring electrodes to affect the electrooxidation or electroreduction of the analyte.
  • the hydrophilic article includes a chemical reagent for reacting with the test analyte to produce the electrochemical signal that represents the presence of the analyte in the sample fluid.
  • the reagent may be located in one or more of the landing zone, the detection zone, or at a location along the fluid transport channel.
  • the reagent may be coated on, or present within one or more surfaces defining the landing zone, the detection zone, or the fluid transport channel.
  • the reagent can include a variety of active components selected to determine the presence and/or concentration of various analytes. The test chemistry is therefore selected in respect to the analyte to be assessed. The selection of an appropriate chemistry, such as one or more enzymes, co-enzymes, and co-factors is well within the skill in the art.
  • hydrophilic films of the present disclosure can also be used in the manufacture of microfluidic devices to assist with fluid movement within and along the device via capillary flow action.
  • An exemplary microfluidic device is described in U.S. Patent No. 6,375,871 ("Methods of Manufacturing Microfluidic Articles").
  • Such devices may comprise capillary channels within a base or spacer layer which is covered with a hydrophilic film.
  • Such devices can be used for purification or analysis of chemical or biological components.
  • microfluidic devices examples include but are not limited to sample preparation, cell sorting, capture, and detection, colorimetric or fluorescent detection assays, nucleic acid analysis, immunoassays, blood chemistry analysis, temperature controlled biological reactions such as polymerase chain reaction (PCR).
  • PCR polymerase chain reaction
  • wells 160 and 165 Another feature that may be present in the fluid transport channels of some embodiments of the present disclosure are illustrated by wells 160 and 165.
  • Such wells may contain a component that reacts with or otherwise alters a property of the fluid being transported, e.g., one or more of chemical reagents.
  • a component may be held within the well and/or coated or otherwise applied to an exposed surface of the well.
  • the component may not be present in the well until use, e.g., the component can be injected into the well.
  • the well may be located upstream of the detection zone.
  • well 165 is located upstream of detection zone 175.
  • Fluid entering fluid transport channel 140 at landing zone 150 will be transported along hydrophilic layer 120 to well 165.
  • the fluid will contact any component present within the well.
  • the fluid will then continue traveling by capillary action into detection zone 175, where features of the fluid, including features potentially modified by the component, may be detected.
  • the combination of the component on well 160 with the fluid may occur in detection zone 170.
  • fluid is transported from landing zone 150 to detection zone 170.
  • a component is independently transported, e.g., moved from well 160 into detection zone 170, where it reacts or otherwise interacts with the fluid.
  • features of the fluid including features potentially modified by the component, may be detected.
  • detection zones 170 and 175 and/or wells 160 and 165 may include a variation in the general cross-section of fluid transport channel 140.
  • detection zone 170 and 175 are illustrated as cubes, while wells 160 and 165 are illustrated as cylinders.
  • the detection zones and or wells can be of any desired shape, and may or may not include any variation in the cross-section of the fluid transport channel.
  • FIGS. 4 and 5 illustrate cover layer 180, another optional feature that may be beneficial in some embodiments of the present disclosure.
  • it may be desirable to minimize or prevent access to the fluid transport channel.
  • access to the channel may be restricted to certain specific location such as the landing zone.
  • Cover layer 180 illustrates one potential means to prevent undesired contact with the fluid transport layer.
  • cover layer 180 is in contact with the surface of spacer layer 130, opposite hydrophilic layer 120.
  • cover layer 180 covers all or substantially all of spacer layer 130.
  • the cover layer may only cover portions of the spacer layer, e.g. the cover layer may cover all or select portions of fluid transport channel 140, contacting the spacer layer to the extent necessary or desired to maintain its position.
  • the cover layer may be positioned so as to leave portions of the fluid transport channel exposed, e.g., at one or more of a landing zone, a well or a detection zone.
  • all or a portion of the cover layer may be releasably attached to the spacer layer.
  • the entire cover layer may be removed when desired, e.g., just prior to use.
  • select portions of the cover layer may be removed when desired.
  • a portion of the cover layer may be removed to expose one or more of a landing zone, a well, or a detection zone.
  • cover layer may be any suitable material including, e.g., paper, polymeric films, woven and nonwoven webs, metal foils, multilayer constructions and the like, including combinations thereof.
  • the cover layer may be a hydrophilic film.
  • the cover layer may be the same or similar to hydrophilic layer 120.
  • cover layer 180 may include a substrate with hydrophilic layer 120 adhered, directly or indirectly to a substrate and positioned relative to the spacer layer such that the hydrophilic layer forms a boundary of the fluid transport channel.
  • the cover layer should not substantially interfere with detection means.
  • the cover layer should permit sufficient transmission of the appropriate frequency of light to permit detection.
  • FIG. 6 illustrates an edge view of yet another exemplary embodiment of the hydrophilic articles of the present disclosure.
  • Hydrophilic article 300 comprises first substrate 110, hydrophilic layer 120, and second substrate 390 comprising spacer layer 330 and cover layer 380.
  • spacer layer 330 is integral to cover layer 380.
  • substrate 390 may be modified, e.g., embossed, etched, ground, molded, etc., to form fluid transport channels 340 in substrate 390.
  • the modified region below dashed line A-A is referred to as the spacer layer, while the unmodified region is referred to as the cover layer.
  • Hydrophilic layer 120 is adhered to spacer layer 330 such that fluid transport channels 340 are bounded on one side by the hydrophilic layer.
  • second substrate 390 may be bonded, directly or indirectly, to hydrophilic layer 120.
  • the hydrophilic layer comprises acidified, sintered silica nanoparticles such as those described in U.S. Publication 2010/0035039 ( U.S. Application No. 12/187977, filed August, 7, 2008 , "Acicular Silica Coating for Enhanced Hydrophilicity/Transmissivity").
  • nanoparticles means particles having a major dimension of no greater than 200 nm, e.g., no greater than 150 nm, no greater than 100 nm, or even no greater than 50 nm.
  • the nanoparticles comprise substantially spherical nanoparticles, i.e., nanoparticles having a ratio of major dimension to minor dimension of no greater than 2, in some embodiments, no greater than 1.5, or even no greater than 1.2.
  • the substantially spherical nanoparticles have an average diameter of no greater than 50 nm, no greater than 40 nm, no greater than 20 nm, no greater than 10 nm, or even no greater than 5 nm.
  • a multimodal distribution of spherical nanoparticles may be used.
  • such multimodal distributions include at least one peak having an average diameter of no greater than 40 nm.
  • Such multimodal distributions include at least peak, and in some embodiments multiple additional peaks having an average diameter of greater than 40 nm, e.g., greater than 100 nm, greater than 200 nm, or even greater than 300 nm.
  • such multimodal distributions include at least 1 wt.% of nanoparticles in the at least one peak having an average diameter of no greater than 40 nm, e.g., at least 5 wt.% or even at least 10 wt.%.
  • the nanoparticles comprise elongated nanoparticles.
  • the elongated nanoparticles have a ratio of length to average cross-sectional diameter of at least 2, in some embodiments, at least 3, at least 5, or even at least 10.
  • the ratio of length to average cross-sectional diameter is no greater than 20, e.g., no greater than 15.
  • the ratio of length to average cross-sectional diameter ranges from 2.5 to 20, inclusive, e.g., 3 to 15, inclusive.
  • the hydrophilic layer comprises only substantially spherical nanoparticles. In some embodiments, only elongated nanoparticles may be used. However, as illustrated in FIGS. 1 to 3 , in some embodiments, hydrophilic layer 120 incorporates both substantially spherical nanoparticles 122 and elongated nanoparticles 124. In some embodiments, the hydrophilic layer contains at least 30 wt.%, e.g., at least 40 wt.%, at least 50 wt.% or even at least 60 wt.% substantially spherical nanoparticles, based on the total weight of nanoparticles.
  • the hydrophilic layer comprises at least 2 wt.%, e.g., at least 5 wt.%, at least 10 wt.%, at least 30 wt.%, or even at least 50 wt.% elongated nanoparticles, based on the total weight of nanoparticles.
  • the hydrophilic layer comprises 40 to 98 wt.%, e.g., 50 to 95 wt.%, inclusive spherical nanoparticles and, correspondingly, 2 to 60 wt.%, e.g., 5 to 50 wt.% elongated nanoparticles.
  • the silica nanoparticles are substantially free of organic surface modifying agents, i.e., organic compounds ionically or covalently bonded to the surface of the silica nanoparticles.
  • organic surface modifying agents i.e., organic compounds ionically or covalently bonded to the surface of the silica nanoparticles.
  • the unmodified silica nanoparticles of the present disclosure are substantially free of such materials, i.e., if present at all, the surface modifier loading is no greater than 5% of the theoretical loading required for 100% surface coverage, e.g., less than 2%, or even less than 1% of such theoretical loading.
  • the silica nanoparticles are free of any organic surface modifying agents.
  • the hydrophilic layer can be prepared by acidifying the silica nanoparticles in a coating solution, applying the coating solution to the surface of a substrate, and drying the coating to provide a hydrophilic layer comprising acidified, sintered silica nanoparticles.
  • Inorganic silica nanoparticles in aqueous media are well known in the art and available commercially.
  • Silica sols in water or aqueous alcohol solutions are available commercially under such trade names as LUDOX (manufactured by E.I.
  • Non-aqueous silica sols also called silica organosols
  • silica sol dispersions wherein the liquid phase is an organic solvent.
  • Such organosols are available from Nissan Chemical.
  • the coating composition may be acidified to the desired pH level with an acid having a pKa (H 2 O) of less than 5, in some embodiments, less than 2.5, e.g., less than 1.
  • Useful acids include both organic and inorganic acids and may be exemplified by oxalic acid, formic acid, H 2 SO 3 , H 3 PO 4 , CF 3 CO 2 H, HCl, HBr, HI, HBrO 3 , HNO 3 , HClO 4 , H 2 SO 4 , CH 3 SO 3 H, CF 3 SO 3 H, CF 3 CO 2 H, and CH 3 OSO 2 OH.
  • preferred acids include HCl, HNO 3 , H 2 SO 4 , and H 3 PO 4 .
  • the coating composition generally contains sufficient acid to provide a pH of less than 5, in some embodiments, less than 4, or even less than 3.
  • a porous network of silica nanoparticles is obtained by acid sintering of the agglomerated silica nanoparticles as the water or solvent evaporates and the acid concentration increases. Electron micrographs reveal such bonds as silica "necks" between adjacent particles which are created by the acid in the absence of silica sources such as tetraalkoxysilanes or siloxane oligomers. Their formation is attributed to the catalytic action of strong acid in making and breaking siloxane bonds.
  • the silica nanoparticles can be sintered with a heat treatment (e.g., flame treatment).
  • Heat treatment can be conducted, for example, by passing the structured substrate under a flame (burner) for typically about 1-3 seconds, or even longer provided the substrate is not subjected to conditions that melt the substrate.
  • Other techniques of heating may also include, for example, infra-red heaters, and hot air blowers.
  • the surface opposite the coated surface can be cooled, for example, by a chilled metal roll or via liquid application to enable longer residence times under the flame.
  • the coatings of the present invention are applied to achieve a uniform average dry thickness between 50 and 1000 nm, inclusive, preferably 75 to 400 nm, and more preferably 100 to 300 nm, inclusive, as measured using an ellipsometer such as a Gaertner Scientific Corp Model No. L115C.
  • compositions may be coated on the article using conventional techniques, such as bar, roll, curtain, rotogravure, spray, or dip coating techniques.
  • conventional techniques such as bar, roll, curtain, rotogravure, spray, or dip coating techniques.
  • it may be desirable to oxidize the substrate surface prior to coating using corona discharge or flame treatment methods.
  • Other methods capable of increasing the surface energy of the article include the use of primers.
  • the articles of the disclosure include a substrate bearing a continuous network of silica particle agglomerates.
  • continuous refers to covering the surface of the substrate with virtually no discontinuities or gaps in the areas where the gelled network is applied. Thus, e.g., if the silica particles are pattern-coated, uncoated regions may be created, yet the coating would be considered “continuous” provided there were virtually no discontinuities or gaps in the areas where the gelled network is applied.
  • network refers to an aggregation or agglomeration of acicular silica particles linked together to form a porous three-dimensional network.
  • the nanoporosity of the sintered nanosilica coating leads to high hydrophilicity, e.g., superhydrophilicity.
  • ASTM D7334-08 an advancing contact angle of less than 45 degrees in indicative of wetting, while advancing contact angles of less than 20 degrees are indicative of excellent wetting.
  • a typical silica glass surface exhibits a water contact angle of 37-43 degrees.
  • the highly porous acid-sintered-nanosilica-coatings exhibit lower water contact angles, e.g., less than 10 degrees, in less than 0.5-2 seconds, in part because of the nanowicking of water into the network of capillaries present in the coatings.
  • the apparent water contact angle of a liquid on a surface is dependent upon the roughness of the surface.
  • the apparent contact angle decreases.
  • the roughness approaches infinity, and any liquid having a contact angle of less than 90 degrees on a smooth surface, will have a contact angle approaching zero on a nanoporous surface resulting in complete wetting of the nanoporous surface.
  • a resin e.g., a polymeric resin
  • the hydrophilic layer comprises no greater than 5 weight percent (5 wt.%) resin, e.g., no greater than 2 wt.%, or even substantially no resin, based on the total weight of the hydrophilic layer.
  • substantially no resin means that the hydrophilic layer is free of resin except for any trace amounts that may be present due to, e.g., normal material supply and manufacturing processes.
  • the hydrophilic layer comprises at least 95 weight percent of the nanoparticles, e.g., at least 98 wt.% nanoparticles based on the total weight of the hydrophilic layer. In some embodiments, the hydrophilic layer consists essentially of the nanoparticles. For example, in some embodiments, the hydrophilic layer comprises at least 95 weight percent of the nanoparticles and no greater than 5 wt.% resin, e.g., at least 98 wt.% nanoparticles and no greater than 2 wt.% resin, based on the total weight of the hydrophilic layer.
  • hydrophilic articles of the present disclosure may be used to transport fluids, including, e.g., biological fluids.
  • biological fluids include blood, urine, sweat, and saliva.
  • silica-SPH was a substantially spherical colloidal silica having a average diameter of 4 nm (NALCO 1115, available from Nalco, Naperville, Illinois).
  • SILICA-ELG was an elongated colloidal silica having a diameter of 9-15 nm and a length of 40-100 nm (SNOWTEX OUP, available from Nissan Chemical, Houston, Texas).
  • a sample film was conditioned at 23 °C / 50% RH (relative humidity) for eight hours before and during testing.
  • the film sample was placed on a clean flat horizontal surface with the side to be tested facing up.
  • a 3 microliter drop of deionized water containing 0.07% by weight Wool Fast Brilliant Red R.L. Dye, (Pylam Products, Garden City, New York) was gently placed on the surface with a micropipette. The drop was allowed to spread to its maximum extent and completely dry.
  • the diameter of the dyed area was determined by placing the film over a paper with premeasured circles of varying diameters. The average drop diameter was recorded.
  • Example 1 A silica coating solution was prepared by combining 70 weight percent of SILICA-SPH with 30 weight percent of SILICA-ELG. A suspension was prepared by mixing 2 to 3 weight % of the resulting combined silica composition with 97 to 98 weight percent water. Nitric acid (commercial grade, obtained from EMD, Gibbstown, New Jersey) was added to adjust the pH of the silica coating to 2.5.
  • the silica coating was applied to a PET film (0.09 mm thick polyethylene terephthalate film, 3M Company, St. Paul, Minnesota) using a slot-fed die. The coating was dried at about 130 °C, yielding a dried coat weight of 0.3 to 0.4 grams per square meter.
  • the coated film of Example 1 (EX-1) and was subjected to the Contact Angle Procedure and the Spreading Drop Procedure. The results are summarized in Table 1, and compared to results obtained using the same PET, but uncoated (CE-1).
  • Table 1 Contact angle and spreading drop results for examples EX-1 and CE-1.
  • Example 1 The sample of Example 1 was subjected to several conditions to assess the durability of the coatings. The results were compared to a commercially available hydrophilic film comprises a PET substrate with a conventional organic hydrophilic coating (3MTM Hydrophilic Polyester Film 9962, "CE-2"). Film samples were immersed into either a 25 °C or a 90 °C water bath for five minutes. Once dried, the contact angle was measured. Mean result for replicate measurements on the films of EX-1 and CE-2 are shown in Table 2. Table 2: Contact angle (degrees) for EX-1 and CE-1. Test EX-1 CE-2 Contact Angle Contact Angle Before After Before After Water Immersion 25 °C 8.2 11 14.2 43 90 °C 8.2 13 14.2 59
  • the hydrophilic layer retains its hydrophilic properties after immersion in water.
  • a device comprising a hydrophilic surface which retains its hydrophilic properties after exposure to liquids is that the surface chemistry does not solubalize and contaminate the test fluid.
  • a fluid transport device comprising a reusable hydrophilic layer is that fluid can pass over the film multiple times and fluid flow will not be compromised, such as in lab-on-a-chip assays involving but not limited to washing or fluid separation steps.
  • the hydrophilic coating in this invention retained its hydrophilic properties after immersion in 90 degree Celsius water, which is advantageous for use in devices which require elevated temperatures for analyte testing such as polymerase chain reaction.
  • EX-1 was also evaluated for resistance to wiping (abrasion) by applying 3 or 10 wipes with a tissue (KIMTECH wipes, available from Kimberly-Clark Corporation, Irving, Texas). After wiping, contact angle and spreading drop were measured. Finally, accelerated stability of EX-1 was assessed by placing the example films in chambers held at 24 °C/60% Relative Humidity ("60% RH") and 49 °C/dry for 8 weeks. Afterward, contact angle and spreading drop were measured. Mean result for replicate measurements are shown in Table 3. Table 3: Contact angle and spreading drop results for EX-1.

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Claims (21)

  1. Article hydrophile (100) comprenant un substrat (110), une première surface d'une couche hydrophile (120) comprenant des nanoparticules frittées de silice acidifiée (122, 124) fixées au substrat, et une couche d'espacement (130) fixée à une première partie d'une deuxième surface de la couche hydrophile (120) opposée à la première surface, dans lequel la couche d'espacement (130) définit au moins un canal de transport de fluide (140) délimité sur un côté par une deuxième partie de la deuxième surface de la couche hydrophile, et dans lequel la couche hydrophile contient moins de 0,002 pour cent en poids d'agent tensioactif, sur la base du poids total de la couche hydrophile.
  2. Article hydrophile selon la revendication 1, dans lequel la couche hydrophile (120) ne comprend pas plus de 0,001 pour cent en poids d'agent tensioactif, sur la base du poids total de la couche hydrophile.
  3. Article hydrophile selon la revendication 2, dans lequel la couche hydrophile (120) ne comprend pas plus de 0,0005 pour cent en poids d'agent tensioactif, sur la base du poids total de la couche hydrophile.
  4. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel le canal de transport de fluide (140) comprend une zone de réception (150) comprenant une partie exposée de la couche hydrophile (120).
  5. Article hydrophile selon la revendication 4, dans lequel la zone de réception (150) se situe au niveau d'un bord du substrat (110).
  6. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel le canal de transport de fluide (140) comprend une zone de détection (170, 175) comprenant une partie de la couche hydrophile (120) qui est (i) exposée ou (ii) couverte par une couche ayant une transmissivité d'au moins 50 % pour au moins une longueur d'onde d'énergie électromagnétique entre 200 et 800 nm, inclus.
  7. Article hydrophile selon la revendication 6, dans lequel l'article (100) comprend la zone de réception (150), et dans lequel la zone de détection (170, 175) est en communication fluidique avec la zone de réception via le canal de transport (140).
  8. Article hydrophile selon l'une quelconque des revendications précédentes, comprenant en outre une couche de couverture (180) en contact avec au moins une partie d'une surface de la couche d'espacement (130) opposée à la couche hydrophile (120) et couvrant au moins une partie du canal de transport de fluide (140).
  9. Article hydrophile selon la revendication 8, dans lequel la couche de couverture (180) comprend une deuxième couche hydrophile comprenant des nanoparticules frittées de silice acidifiée fixées à un deuxième substrat (390).
  10. Article hydrophile selon la revendication 8, dans lequel la couche de couverture (180) est solidaire de la couche d'espacement (130).
  11. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel les nanoparticules comprennent des nanoparticules allongées de silice (124) ayant un rapport de la longueur moyenne au diamètre d'au moins 2.
  12. Article hydrophile selon la revendication 11, dans lequel le rapport de la longueur moyenne au diamètre des nanoparticules allongées de silice (124) va de 3 à 15.
  13. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel les nanoparticules comprennent des nanoparticules de silice sensiblement sphériques (122) ayant un rapport du diamètre maximal au diamètre minimal inférieur à 2.
  14. Article hydrophile selon la revendication 13, dans lequel le rapport du diamètre maximal au diamètre minimal des nanoparticules de silice sensiblement sphériques (122) est inférieur à 1,2.
  15. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel les nanoparticules comprennent 50 à 95 pour cent en poids de nanoparticules de silice sensiblement sphériques (122) ayant un rapport du diamètre maximal au diamètre minimal inférieur à 2, et 5 à 50 parties en poids de nanoparticules allongées de silice (124) ayant un rapport de la longueur moyenne au diamètre d'au moins 2, sur la base du poids total des nanoparticules.
  16. Article hydrophile selon la revendication 15, dans lequel le rapport du diamètre maximal au diamètre minimal des nanoparticules de silice sensiblement sphériques (122) est inférieur à 1,2 et le rapport de la longueur moyenne au diamètre des nanoparticules allongées de silice (124) va de 3 à 15.
  17. Article hydrophile selon la revendication 15 ou 16, dans lequel les nanoparticules comprennent 60 à 80 pour cent en poids des nanoparticules sensiblement sphériques (122) et 20 à 40 parties en poids des nanoparticules allongées (124), sur la base du poids total des nanoparticules.
  18. Article hydrophile selon l'une quelconque des revendications précédentes, dans lequel la couche hydrophile (120) comprend au moins 95 pour cent en poids des nanoparticules (122, 124), sur la base du poids total de la couche hydrophile.
  19. Article hydrophile selon la revendication 18, dans lequel la couche hydrophile (120) ne comprend pas plus de 2 pour cent en poids de résine, sur la base du poids total de la couche hydrophile.
  20. Procédé de transport d'un fluide avec l'article hydrophile (100) selon l'une quelconque des revendications précédentes comprenant : l'application du fluide à une première région de la deuxième partie de la deuxième surface de la couche hydrophile (120) et l'absorption capillaire du fluide au sein du canal de transport de fluide (140) de la première région à une deuxième région de la deuxième partie de la deuxième surface de la couche hydrophile (120).
  21. Procédé selon la revendication 20, dans lequel le fluide est un fluide biologique.
EP12783802.7A 2011-11-02 2012-10-30 Dispositif hydrophile de transport de fluide Active EP2773706B1 (fr)

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US201161554553P 2011-11-02 2011-11-02
PCT/US2012/062583 WO2013066874A1 (fr) 2011-11-02 2012-10-30 Dispositif de transport de fluide hydrophile

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EP3134466B1 (fr) 2014-04-24 2022-06-01 3M Innovative Properties Company Films de regulation de fluide avec des surfaces hydrophiles, procédés de fabrication et processus de nettoyage des surfaces structurées
WO2016094715A2 (fr) * 2014-12-10 2016-06-16 Berkeley Lights, Inc. Déplacement et sélection de micro-objets dans un appareil micro-fluidique
EP3429750A1 (fr) * 2016-03-15 2019-01-23 Evonik Röhm GmbH Dispositifs microfluidiques ayant un microcanal à revêtement hydrophile
WO2019046696A1 (fr) 2017-09-01 2019-03-07 3M Innovative Properties Company Capteur et système de détection pour procédé de test d'ajustement de respirateur
CN111051869A (zh) * 2017-09-01 2020-04-21 3M创新有限公司 用于呼吸器的感测元件
CN111050644A (zh) 2017-09-01 2020-04-21 3M创新有限公司 用于呼吸器的感测系统
EP3675970A4 (fr) 2017-09-01 2021-06-30 3M Innovative Properties Company Procédé d'essai de réglage pour respirateur doté d'un système de détection
CN108375399B (zh) * 2018-03-20 2024-10-18 苏州原位芯片科技有限责任公司 流量传感器
JP7347931B2 (ja) * 2018-12-26 2023-09-20 スリーエム イノベイティブ プロパティズ カンパニー マイクロ流体デバイス用フィルム、マイクロ流体デバイス及びその製造方法
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CN104169378A (zh) 2014-11-26
US9383294B2 (en) 2016-07-05
EP2773706A1 (fr) 2014-09-10
US20140299193A1 (en) 2014-10-09
CN104169378B (zh) 2018-04-13
WO2013066874A1 (fr) 2013-05-10
TW201328876A (zh) 2013-07-16
BR112014011270A2 (pt) 2017-05-02

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